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1、10.6.18A(J&WScientific,91BlueRavineRd,Folsom,CA95630-4714,AOACOfficialMethod2000.05USA);orequivalent].A4mmid,singleordoublerestrictor-type(1-DeterminationofGlyphosateandor2-piece)inletliner,packedwitha1cmlongplugofsilanizedglassAminomethylphosphonicAci
2、d(AMPA)inCropswoolorfusedsilicawool,ispositionedinthemiddleoftheliner.GasChromatographywithMass-SelectiveDetectionPlacetheinletendofthecolumnwithintheinletliner,6–8mmfromFirstAction2000thebottomrestrictoroftheinletliner.Hecarriergasflowrate:ca30cm/sat1
3、80°C;equaltoabout40–50kPa(6–7psi)atcolumn(Themethodisapplicabletothedeterminationofglyphosateandhead.Temperatureprogram:initialtemperature,holdat90°Cfor1.5aminomethylphosphonicacidincropsat0.050–2.0mg/kg.)min,increaseto300°Cat30°C/min(20°C/miniflimited
4、byinstru-SeeTables2000.05Aand2000.05Bforresultsofthementcapabilities),andholdat300°Cfor4min.Analternativepro-interlaboratorystudysupportingacceptanceofthemethod.gramforincreasedresolutionis:initialtemperature,holdat60°CforA.Principle1.5min,increaseto12
5、0°Cat10°C/min,holdat120°Cfor1.0min,increaseto300°Cat30°C/min,andholdat300°Cfor4min.Injec-Glyphosateandaminomethylphosphonicacid(AMPA)residuestionporttemperature:200°C.MSDinterfacetemperature:280°C.areextractedfromcropsbymacerationwithwater.Thecrudeex-t
6、ractispartitionedwithmethylenechlorideandthensubjectedtoaInjectionvolume:2–5mL,dependingonanalytedetectability.Inletcation-exchange(CAX)procedure.Theanalytesinthepurifiedex-system:operatedinthesplitlessmode,withtheinletpurged1.0mintractarederivatizeddi
7、rectlywithamixtureoftrifluoroaceticanhy-afterinjection.(Note:Sensitivitymaybeoptimizedbyadjustingthedrideandheptafluorobutanol.Theaminefunctionalgroupsareinitialoventemperaturebetween60and90°C.Adjustingotherpro-derivatizedtoformthecorrespondingtrifluor
8、oacetylderivatives.gramvariablessuchasintermediateholdtemperatureanddurationThecarboxylicandphosphonicacidfunctionalgroupsaremayalsobehelpful.)derivatizedtoformthecorrespondingheptafluorobutylesters.After(b)Mass-selectivedetector.—Aquad
